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IS 228-12 (2001): Methods of chemical analysis of steels,Part 12: Determination of manganese by periodatespectrophotometric method in low and high alloy steels (formanganese 0.01 to 5.0 percent) [MTD 16: Alloy Steels andForgings]

~mm

METHODS

W’laGl’ W fmtw (0.01a 5.0 m?l’?i m * W) q

( ak7rg@t@r)

Indian Standard

OF CHEMICAL ANALYSISOF STEELS

PART 12 DETERMINATION OF MANGANESE BY PERIODATE SPECTROPHOTOMETRICMETHOD IN PLAIN CARBON, LOW ALLOY AND HIGH ALLOY STEELS

(FOR MANGANESE 0.01 TO 5.0 PERCENT)

( Fourth Revision)

ICS 77.080.20.,

.

.,

0 BIS 2001

June 2001

BUREAU OF IN DIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

IMce Group 1

Methods of Chemical Analysis of Ferrous Metals Sectional Committee, MTD 2

FOREWORD

This Indian Standard (Part 12) (Fourth Revision) was adopted by the Bureau of Indian Standards, after thedraft finalized by the Methods of Chemical Analysis of Ferrous Metals Sectional Committee had been approvedby the Metallurgical Engineering Division Council.

IS 228, which was first published in 1952 and subsequently revised in 1959, covered the chemical analysis ofplain carbon and low alloy steels along with pig iron and cast iron. It was again revised to make it comprehensivein respect of steel analysis and to exclude pig iron and cast iron which were being covered in separate standards.During its second revision the standard has been split up in several parts.

This part covers the method for determination of manganese in plain carbon, low alloy and high alloy steels byperiodate spectrometric method. The other parts of this series are:

Part 1:1987

Part 2:1987

Part 3:1987

Part 4:1987

Part5 :1987

Part 6:1987

Part 7:1990

Part 8:1989

Part 9:1989

Part 10:1989

Part 11:1990

Part 13:1982

Part 14:1988

Part 15:1992

Part 16:1992

Part 18:1998

Part 19:1998

Methods for chemical analysis of steels — Determination of carbon by volumetric method(for carbon 0.05 to 2.50 percent) (third revision)

Determination of manganese in plain carbon and low alloy steels by arsenite method (thirdrevision)

Determination of phosphorus by alkalimetric method (third revision)

Determination of total carbon by gravimetric method (for carbon greater than or equal to 0.1percent) (third revision)

Determination of nickel by dimethyl glyoxime (gravimetric) method (for nickel greater thanor equal to 0.1 percent) (Wrd revision)

Determination of chromium by persulphate oxidation method (for chromium greater thanor equal to 0.1 percent) (third revision)

Determination of molybdenum by alpha-benzoinoxime method (for molybdenum 1percent)(third revision)

Determination of silicon by the gravimetic method (for silicon 0.05 to 0.50 percent) (thirdrevision)

Determination of sulphur in plain carbon steels by evolution method (for sulphur 0.01 to0.25 percent) (third revision)

Determination of molybdenum by thoicyanate (photometric) method in low and high alloysteels (for molybdenum 0.01 to 1.5 percent) (third revision) ,

Determination of silicon by reduced molybdosilicate spectrophotometric in carbon steelsand low alloy steels for silicon 0.01 to 0.05 percent) (third revision)

Determination of arsenic

Determination of carbon by thermal conductivity method (for carbon 0.005 to 2.000 percent)

Determination of copper by thiosulphate iodide method (for copper 0.05 to 5 percent)

Determination of tungsten by spectrophotometric method (for tungsten 0.1 to 2 percent)

Determination of oxygen by instrumental method

Determination of nitrogen by steam distillation

During this revision the method for determination of manganese in high alloy steels have been included and theperiodate spectrometric method specified in the standard has been updated.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2:1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained inthe rounded off value should be the same as that of the specified value in this standard.

IS 228 (Part 12): 2001

Indian Standard

METHODS FOR CHEMICALOF STEELS

ANALYSIS

PART 12 DETERMINATION OF MANGANESE BY PERIODATE SPECTROPHOTOMETRICMETHOD IN PLAIN CARBON, LOW ALLOY AND HIGH ALLOY STEELS

(FOR MANGANESE 0.01 TO 5.0 PERCENT)

(Fourth Revision)

1 SCOPE

This standard (Part 12) describes the method for thedetermination of manganese in plain carbon, low alloyand high alloy steels in the range of 0.01 to 5.0 percentby periodate spectrophotometric method.

2 REFERENCES

The following Indian Standards contain provisionswhich through reference in this text, constituteprovision of this standard. At the time of publication,the editions indicated were valid. All standards aresubject to revision , and parties to agreements basedon this standard are encouraged to investigate thepossibility of applying the most recent editions of thestandards indicated below.

IsNo. Title264:1976 Nitric acid (second revision)

266:1993 Sulphuric acid (third revision)

1070:1992 Reagent grade water (third revision)

3 SAMPLING

The samples shall be drawn and prepared as describedin the relevent Indian Standard specification.

4 QUALITY OF REAGENTS

Unless specified otherwise, analytical grade reagentsand reagent grade water (see IS 1070) shall beemployed for the test.

5 DETERMINATION OF MANGANESE

5.1 Outline of the Method

After dissolution of the sample in sulphuric-phosphoric acid mixture and nitric acid, the solution isfumed with perchloric acid. Manganese is oxidized topermanganic acid by potassium periodate.Absorbance of the solution is measured at 545 nm.

5.2 REAGENTS

5.2.1 Sulplmric-Phosphoric Acid Mixture—Add 100ml of sulphuric acid (rd=l .84) (IS 266) and 150 ml of

phosphoric acid (rd=l .75) to 600 ml water. Cool anddilute to 1 Iitre with water.

5.2.2

5.2.3

5.2.4

5.2.5

Nitric Acid (rd=l .42) — Conforming to IS 264.

Perchloric Acid, 70 percent.

Dilute Perchloric Acid, 1:99 (v/v).

Potassium Periodate Solution

Dissolve 7.5 g of potassium periodate in 200 ml ofdilute nitric acid (1 : 1) with warming. Add 400 ml ofphosphoric acid, cool and dilute to 1 Iitre.

5.2.6 Standard Manganese Solution (1 ml= 0.1 mgMn)

Prepare as described in Method A or B.

5.2.6.1 Method A (Preparation from manganesemetal)

Take 0.1 g of manganese metal (purity 99.8 percent)in a beaker and add 10 ml of dilute nitric acid (1 : 1).Heat gently until dissolution is complete and brownfumes are expelled. Cool, transfer to 1 litre volumetricflask, dilute to volume and mix.

5.2.6.2 Method B (Preparation from potassiumpermanganate)

Dissolve 3.2 g of potassium permanganate in 1 litreof water. Let it stand in the dark for two weeks. Filterwithout washing through a Gooch crucible. Avoidcontact with rubber or other organic material. Store ina dark coloured glass stoppered bottle.

5.2.6.3 Standardization

Dry a portion of sodium oxalate at 105° C. Transfer0.3000 g of sodium oxalate to 500 ml beaker. Add250 ml of dilute sulphuric acid (1 : 19), previouslyboiled for 10 to 15 min and then stir until the oxalatehas dissolved. Add about 40 ml of potassiumpermanganate solution while stirring slowly. Let itstand until the pink colour disappears. Heat to55°C to 60°C and complete the titration by addingpotassium permanganate solution until faint pink

1

IS 228 (Part 12) :2001

colour persists for 30 s. Find out the normality of thesolution and adjust to 0.1 N.Transfer 90 ml of 0.1 N potassium permanganatesolution to 500 ml beaker and add 10 ml of dilutesulphuric acid (1 : 1). Reduce the potassiumpermanganate solution by sulphurous acid and boil thesolution until free of sulphurdioxide. Cool and transferto 1 Iitre volumetric flask and make up.

5.3 Procedure

5.3.1 Select sample as per Table 1. The dilutions andalequots to be pipetted out are also given in Table 1.

Table 1 Sample Selection

Mn Weight Dilution Aliquot(%) (g) (ml) (ml)(1) (2) (3) (4)

0.01to0.05 1.0 50 20>0.05 to 0.1 1.0 100 20>0,1 to 0.5 0.5 100 20>0.5 to 2.5 1.0 500 10>2.5 to 5.0 0.5 500 10

Add 8 to 10 ml HC1 (1 : 1). Add enough HN03 tohasten dissolution, add 3 to 4 ml in excess. Add 10 mlHCI04, evoporate to fumes to oxidize chromium andexcess HC1. Continue fuming till salts separate.Cool, add 50 ml water, digest transfer to a 50,100 or500 ml flask. Dilute to volume, mix, allow insolublematter to settle and filter through a dry filter. Discardthe first 15 to 20 ml filterate.

Transfer 10 or 20 ml portions and specified in Table 1to two 50 ml flasks.

To one, add 10 ml IU03 and heat to less than 90°C for20 to 30 min. Dilute to volume and mix.

To another add 10 ml nitric/phosphoric acid mixure,heat the solution at not less than 90”C for 20 to 30 min.Cool and d~lute to volume. Take the absorbancereadings of first against second.

NOTES1 A boiling water bath in which the flasks can be immerse~may be used.

2 The water used for dilution should be pretreated withpotassium periodate.

Convert the spectrophotometeric readings of thesample to milligrams of manganese by means ofcalibration curve and calculate the percentage ofmanganese as given in 5.4.

5.3.2 Blank

Carry out a blank by pipetting out another aliquot ofthe sample in a 250 ml conical flask. Add 5 ml of acidmixture (5.2.1) and boil for 10 min. Cool and proceedas in 5.3.1.

5.3.3 Calibration Curve

Transfer O, 0.5, 1.0, 2.0, 4.0, 5.0 ml of standardmanganese solution (5.2.6) to seven 50 ml volumetricflasks and proceed according to 5.3.1. Draw acalibration curve of absorbance values againstmilligrams of manganese in the various aliquots.

5.4 Calculation

Manganese, percent by mass= $ x O.

where

A = mass in mg, of manganesealiquot of the solution, and

found in

B = mass in g, of the sample represented byaliquot of the solution taken.

5.5 Precision

a)

b)

c)

d)

~ 0.006 percent for manganese content below0.02 perc6nt,~ 0.01 percent for manganese content between0.02 to 0.20 percent,+0.02 percent for manganese content between0.20 to 0.50 percent, and*0.03 percent for manganese content between0.50 to 2.00 percent.

2

Bureau of Indian Standards

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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review”indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc : No. MTD 2 (4112).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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